Gong Suxuan, Bo Tao, Huang Lan, Li Ke An, Liu Huwei
Key Laboratory of Bioorganic Chemistry and Molecular Engineering of the Ministry of Education, College of Chemistry and Molecular Engineering, Peking University, Beijing, PR China.
Electrophoresis. 2004 Apr;25(7-8):1058-64. doi: 10.1002/elps.200305802.
A mixture of six biphenyl nitrile compounds and three related substances with high hydrophobicity and similar structures was successfully separated by microemulsion electrokinetic chromatography (MEEKC) within 30 min. The microemulsion system contained 100 mM sodium dodecyl sulfate (SDS), 80 mM sodium cholate (SC), 0.81% v/v heptane, 7.5% v/v n-butanol, 10% v/v acetonitrile, and 10 mM borate. The addition of SC, organic modifiers, sample preparation, and temperature all showed remarkable effects on the separation. The capacity factor (k) was calculated by using dodecyl benzene as the marker for microemulsion, and the calculated partition coefficient log P(o/w) of the solutes was in the range of 3.35-7.38. The log k values matched well with the log P(o/w) with a correlation coefficient of 0.96. In addition, the linear correlation coefficients of each compound between peak area and concentration were from 0.996 to 0.998 with the repeatability RSD value < 1.2% for migration time and < 4.8% for peak area, and the highest theoretic plate number was > 586000. MEEKC was compared with micellar electrokinetic chromatography (MEKC) indicating that the former method is more suitable for this separation and can be used for the quality control of biphenyl nitrile compounds in the synthesis of liquid crystals.
通过微乳液电动色谱法（MEEKC）在30分钟内成功分离了六种具有高疏水性且结构相似的联苯腈化合物与三种相关物质的混合物。该微乳液体系包含100 mM十二烷基硫酸钠（SDS）、80 mM胆酸钠（SC）、0.81% v/v庚烷、7.5% v/v正丁醇、10% v/v乙腈和10 mM硼酸盐。SC的添加、有机改性剂、样品制备和温度对分离均显示出显著影响。以十二烷基苯作为微乳液的标记物计算容量因子（k），溶质的计算分配系数log P(o/w)在3.35 - 7.38范围内。log k值与log P(o/w)匹配良好，相关系数为0.96。此外，各化合物的峰面积与浓度之间的线性相关系数在0.996至0.998之间，迁移时间的重复性RSD值< 1.2%，峰面积的重复性RSD值< 4.8%，最高理论塔板数> 586000。将MEEKC与胶束电动色谱法（MEKC）进行比较，结果表明前一种方法更适合这种分离，可用于液晶合成中联苯腈化合物的质量控制。
